CN102507279A - Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid - Google Patents
Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid Download PDFInfo
- Publication number
- CN102507279A CN102507279A CN2011103102840A CN201110310284A CN102507279A CN 102507279 A CN102507279 A CN 102507279A CN 2011103102840 A CN2011103102840 A CN 2011103102840A CN 201110310284 A CN201110310284 A CN 201110310284A CN 102507279 A CN102507279 A CN 102507279A
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- Prior art keywords
- sample
- lime stone
- sulfate radical
- chlorion
- solution
- Prior art date
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- 239000006028 limestone Substances 0.000 title claims abstract description 41
- 235000019738 Limestone Nutrition 0.000 title claims abstract description 39
- 239000007787 solid Substances 0.000 title claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title abstract description 5
- 238000002203 pretreatment Methods 0.000 title abstract 2
- 239000000523 sample Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 239000012488 sample solution Substances 0.000 claims abstract description 5
- 241000370738 Chlorion Species 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 12
- 238000004255 ion exchange chromatography Methods 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 238000005374 membrane filtration Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 239000012086 standard solution Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 2
- 238000000120 microwave digestion Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a sample pretreatment method for determining the content of chloride ions and sulfate radicals in limestone solid, which comprises grinding a limestone sample, sieving with a 110 mesh sieve, and sealing in a sample flask; accurately weighing the limestone sample, adding a certain concentration of an acid solution for dissolving the sample to ensure the chloride ions and sulfate radicals to be fully released into the solution, and diluting to a constant volume; and neutralizing the sample solution with a certain concentration of alkali to regulate a pH value to a certain range, performing membrane filtration, and determining the content of chloride ions and sulfate radicals in the sample by ion chromatography. The method has simple process, easy operation, good repeatability, relative standard deviation smaller than 1.68%, and recovery of standard addition above 94.1%.
Description
Technical field
The present invention design belongs to the chemical analysis test technical field, relates to the content of chlorion and sulfate radical in the ion-chromatographic determination slightly solubility solid sample, relates in particular to the mensuration of chlorion and sulfate radical content in the lime stone sample.
Background technology
The lime stone principal ingredient is lime carbonate (CaCO
3).Lime and lime stone are used as building materials in a large number, also are the important source material of many industry.Cement is by mixing such as lime stone and clays, makes through high-temperature calcination.Glass is made through high-temperature fusion by mixing such as lime stone, silica sand, soda ash.Lime stone burns is processed into purer powder lime carbonate, is used as the inserts of rubber, plastics, paper, toothpaste, cosmetics etc.Because the main purposes of lime stone is on building materials, if it is excessive to contain the content of chloride and sulfate in day lime stone, the rainfall meeting is corroded building, thus the life-span that influence is built.Therefore the detection to chlorion in the lime stone and sulfate radical has certain practical significance.
Chlorion in the lime stone and sulfate radical are wrapped in the solid particle, therefore need dissolve sample, can guarantee that the mensuration of chlorion and sulfate radical is accurate.The water pre-treating method that anionic mensuration does not relate in the capacitive solid there are water/leacheate extraction method, Microwave Digestion and pyrohydrolytic method etc.Water/leacheate extraction method wherein can't guarantee that ion to be detected is discharged in the WS fully; Microwave Digestion, this method test efficient is high, and is satisfactory for result, but apparatus expensive; Pyrohydrolytic method, complex operation step is tested consuming time.The present invention selects certain density perchloric acid solution for use; Guarantee that not only chlorion and sulfate radical in the sample are discharged in the solution fully; And in the ion chromatography process, can not cause interference, thereby make the quantitatively more accurate of chlorion and sulfate radical separating of chlorion and sulfate radical.
Summary of the invention
For deficiency and the defective of alleviating prior art, the object of the present invention is to provide a kind of sample-pretreating method of measuring chlorion and sulfate radical content in the lime stone solid.
The present invention adopts following technical scheme to achieve these goals:
The sample-pretreating method of chlorion and sulfate radical content in the mensuration lime stone solid is characterized in that may further comprise the steps:
(1) grinds: the lime stone solid is ground, behind the screen cloth, sample is sealed in the sample bottle excessively;
(2) dissolving: take by weighing the lime stone sample in small beaker, add the 0.5-2mol/L perchloric acid solution, the cover upper surface ware makes sample dissolution;
(3) neutralization: the pH value of regulating sample solution with NaOH is between 7-12;
(4) filter: adopt 0.20-0.24 μ m filtering membrane that sample solution is filtered.
The sample-pretreating method of chlorion and sulfate radical content in the described mensuration lime stone solid is characterized in that: described lime stone solid sample grinds the back and crosses 110 mesh sieves.
The sample-pretreating method of chlorion and sulfate radical content in the described mensuration lime stone solid is characterized in that: the mol ratio of described perchloric acid and institute's solution example is 2-5: 1.
The sample-pretreating method of chlorion and sulfate radical content in the described mensuration lime stone solid is characterized in that: the preferred 0.22 μ m of described filtering membrane.
Beneficial effect of the present invention:
Sample-pretreating method of the present invention is easy, and is easy to operate, and favorable reproducibility, relative standard deviation are all less than 1.68%, and recovery of standard addition is more than 94.1%.
Embodiment
Embodiment 1: accurately take by weighing the lime stone sample of 0.5g through pulverizing, place the 50ml small beaker, add 0.5mol/L perchloric acid solution 10ml, the cover upper surface ware does not stop to shake up, treat sample dissolution after, add secondary deionized water, be settled to 50ml.Get 2 parts of 20ml solution, portion is mark-on not, and portion adds 100mg/l chlorion standard solution 2ml and 1000mg/L sulfate radical standard solution 1ml respectively, and 2 parts of solution all add 1mol/L sodium hydroxide solution 1ml, and pH value reaches 7, is settled to 100ml.
Solution is through 0.22 μ m disposable filtering film; Solid granule is removed, then got into chromatography of ions analysis, thereby wherein the chlorion and the concentration of sulfate radical are measured; And the content and the recovery of chlorion and sulfate radical in the calculation sample, the result sees attached list 1.
The calculating of chlorion and sulfate radical percentage composition in the lime stone sample, by formula carry out (1).
Recovery of standard addition by formula (2) carries out.
In the formula: chlorion and sulfate radical percentage composition in the X-lime stone solid;
-chlorion recovery of standard addition
-sulfate radical recovery of standard addition
-m
iThe sampling amount of-carbon-lime stone solid, g; c
iChlorion and the sulfate concentration in the mark-on solution not, mg/L; c
I+Chlorion in the mark-on sample and sulfate concentration, mg/L;
Embodiment 2: accurately take by weighing the lime stone sample of 0.5g through pulverizing, place the 50ml small beaker, add 1.0mol/L perchloric acid solution 15ml, the cover upper surface ware does not stop to shake up, treat sample dissolution after, add secondary deionized water, be settled to 50ml.Get 2 parts of 20ml solution, portion is mark-on not, and portion adds 100mg/l chlorion standard solution 2ml and 1000mg/L sulfate radical standard solution 1ml respectively, and 2 parts of solution all add 1mol/L sodium hydroxide solution 2ml, and pH value reaches 8, is settled to 100ml.
Solution is through 0.22 μ m disposable filtering film; Solid granule is removed, then got into chromatography of ions analysis, thereby wherein the chlorion and the concentration of sulfate radical are measured; And the content and the recovery of chlorion and sulfate radical in the calculation sample, the result sees attached list 2.Embodiment 1 is pressed in the calculating of the content of chlorion and sulfate radical and the recovery in the lime stone sample.
Embodiment 3: accurately take by weighing the lime stone sample of 0.5g through pulverizing, place the 50ml small beaker, add 1.5mol/L perchloric acid solution 20ml, the cover upper surface ware does not stop to shake up, treat sample dissolution after, add secondary deionized water, be settled to 50ml.Get 2 parts of 20ml solution, portion is mark-on not, and portion adds 100mg/l chlorion standard solution 2ml and 1000mg/L sulfate radical standard solution 1ml respectively, and 2 parts of solution all add 1mol/L sodium hydroxide solution 5ml, and pH value reaches 10, is settled to 100ml.
Solution is through 0.22 μ m disposable filtering film; Solid granule is removed, then got into chromatography of ions analysis, thereby wherein the chlorion and the concentration of sulfate radical are measured; And the content and the recovery of chlorion and sulfate radical in the calculation sample, the result sees attached list 3.Embodiment 1 is pressed in the calculating of the content of chlorion and sulfate radical and the recovery in the lime stone sample.
Embodiment 4: accurately take by weighing the lime stone sample of 0.5g through pulverizing, place the 50ml small beaker, add 2.0mol/L perchloric acid solution 25ml, the cover upper surface ware does not stop to shake up, treat sample dissolution after, add secondary deionized water, be settled to 50ml.Get 2 parts of 20ml solution, portion is mark-on not, and portion adds 100mg/l chlorion standard solution 2ml and 1000mg/L sulfate radical standard solution 1ml respectively, and 2 parts of solution all add 1mol/L sodium hydroxide solution 10ml, and pH value reaches 12, is settled to 100ml.
Solution is through 0.22 μ m disposable filtering film; Solid granule is removed, then got into chromatography of ions analysis, thereby wherein the chlorion and the concentration of sulfate radical are measured; And the content and the recovery of chlorion and sulfate radical in the calculation sample, the result sees attached list 3.Embodiment 1 is pressed in the calculating of the content of chlorion and sulfate radical and the recovery in the lime stone sample.
Subordinate list 1
A
B
Subordinate list 2
A
B
Subordinate list 3
A
B
Subordinate list 4
A
B
Claims (4)
1. sample-pretreating method of measuring chlorion and sulfate radical content in the lime stone solid is characterized in that may further comprise the steps:
(1) grinds: the lime stone solid is ground, behind the screen cloth, sample is sealed in the sample bottle excessively;
(2) dissolving: take by weighing the lime stone sample in small beaker, add the 0.5-2mol/L perchloric acid solution, the cover upper surface ware makes sample dissolution;
(3) neutralization: the pH value of regulating sample solution with NaOH is between 7-12;
(4) filter: adopt 0.20-0.24 μ m filtering membrane that sample solution is filtered.
2. the sample-pretreating method of chlorion and sulfate radical content in the mensuration lime stone solid according to claim 1 is characterized in that: described lime stone solid sample grinds the back and crosses 110 mesh sieves.
3. the sample-pretreating method of chlorion and sulfate radical content in the mensuration lime stone solid according to claim 1 is characterized in that: the mol ratio of described perchloric acid and institute's solution example is 2-5:1.
4. the sample-pretreating method of chlorion and sulfate radical content in the mensuration lime stone solid according to claim 1 is characterized in that: the preferred 0.22 μ m of described filtering membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110310284.0A CN102507279B (en) | 2011-10-14 | 2011-10-14 | Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110310284.0A CN102507279B (en) | 2011-10-14 | 2011-10-14 | Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102507279A true CN102507279A (en) | 2012-06-20 |
| CN102507279B CN102507279B (en) | 2014-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110310284.0A Expired - Fee Related CN102507279B (en) | 2011-10-14 | 2011-10-14 | Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid |
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| Country | Link |
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| CN (1) | CN102507279B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914600A (en) * | 2012-07-29 | 2013-02-06 | 安徽皖仪科技股份有限公司 | Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography |
| CN106323890A (en) * | 2016-08-19 | 2017-01-11 | 黄婧 | Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process |
| CN106383089A (en) * | 2016-08-29 | 2017-02-08 | 南丹县南方有色金属有限责任公司 | Determination method of calcium and magnesium ions in press-filtrate of zinc smelting purification process |
| CN109060976A (en) * | 2018-07-09 | 2018-12-21 | 德山化工（浙江）有限公司 | Chlorine ion concentration measuring method in silica |
| CN109557237A (en) * | 2019-01-17 | 2019-04-02 | 岭澳核电有限公司 | The measuring method of chlorine ion concentration in containment spray system |
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| CN1502980A (en) * | 2002-11-20 | 2004-06-09 | 河南农大机电技术开发中心 | Combined extractive agent for neutral soil and calcareous soil nutrient |
| CN1975391A (en) * | 2006-12-21 | 2007-06-06 | 中电投远达环保工程有限公司 | Method for measuring chlorion in lime slurry by nitric acid mercurimetry |
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2011
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Patent Citations (2)
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| CN1502980A (en) * | 2002-11-20 | 2004-06-09 | 河南农大机电技术开发中心 | Combined extractive agent for neutral soil and calcareous soil nutrient |
| CN1975391A (en) * | 2006-12-21 | 2007-06-06 | 中电投远达环保工程有限公司 | Method for measuring chlorion in lime slurry by nitric acid mercurimetry |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914600A (en) * | 2012-07-29 | 2013-02-06 | 安徽皖仪科技股份有限公司 | Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography |
| CN102914600B (en) * | 2012-07-29 | 2013-12-11 | 安徽皖仪科技股份有限公司 | Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography |
| CN106323890A (en) * | 2016-08-19 | 2017-01-11 | 黄婧 | Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process |
| CN106383089A (en) * | 2016-08-29 | 2017-02-08 | 南丹县南方有色金属有限责任公司 | Determination method of calcium and magnesium ions in press-filtrate of zinc smelting purification process |
| CN109060976A (en) * | 2018-07-09 | 2018-12-21 | 德山化工（浙江）有限公司 | Chlorine ion concentration measuring method in silica |
| CN109060976B (en) * | 2018-07-09 | 2021-04-30 | 德山化工（浙江）有限公司 | Method for measuring chloride ion concentration in silicon dioxide |
| CN109557237A (en) * | 2019-01-17 | 2019-04-02 | 岭澳核电有限公司 | The measuring method of chlorine ion concentration in containment spray system |
| CN109557237B (en) * | 2019-01-17 | 2021-03-12 | 岭澳核电有限公司 | Method for measuring chloride ion concentration in containment spraying system |
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| Publication number | Publication date |
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| CN102507279B (en) | 2014-01-29 |
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Address after: High tech Zone Wenqu 230088 Hefei Road, Anhui province No. 8 Patentee after: ANHUI WAYEE SCIENCE AND TECHNOLOGY Co.,Ltd. Address before: Tianda high tech Zone 230088 Hefei Road, Anhui province No. 71 Huayi Science Park building B building Anhui instrument Patentee before: ANHUI WAYEE SCIENCE AND TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20220929 Address after: No.8 Wenqu Road, hi tech Zone, Hefei City, Anhui Province Patentee after: Anhui Ketest Testing Co.,Ltd. Address before: No.8 Wenqu Road, hi tech Zone, Hefei City, Anhui Province Patentee before: ANHUI WAYEE SCIENCE AND TECHNOLOGY Co.,Ltd. |
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